CN103477068B - 用于填充风电装置转子叶片中的接缝和缝隙的粘合剂 - Google Patents
用于填充风电装置转子叶片中的接缝和缝隙的粘合剂 Download PDFInfo
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- CN103477068B CN103477068B CN201180062638.2A CN201180062638A CN103477068B CN 103477068 B CN103477068 B CN 103477068B CN 201180062638 A CN201180062638 A CN 201180062638A CN 103477068 B CN103477068 B CN 103477068B
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- polyhydric alcohol
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Abstract
本发明涉及双组分聚氨酯组合物,所述聚氨酯组合物一方面具有较长的晾置时间,并且即使在具有高空气湿度的气候条件下(例如相对空气湿度70%)暴露较长时间之后在40分钟之后、尤其在60分钟之后仍能粘合并且固化成为具有高机械强度的聚合物。所述组合物包括蓖麻油、至少一种具有5~8个羟基的多元醇、基于蓖麻油或者豆油的两种不同聚醚和/或聚酯多元醇的混合物以及多异氰酸酯。所述双组分聚氨酯组合物尤其适合于以力锁合方式填充大面积结构粘合的模制体、尤其是风电装置的转子叶片的侧翼半壳的接缝或缝隙。
Description
技术领域
本发明涉及双组分聚氨酯粘合剂、尤其是结构型双组分聚氨酯粘合剂的领域,并且尤其涉及粘合和填充风电装置转子叶片的接缝和缝隙的领域。
背景技术
长期以来就已应用基于多元醇和多异氰酸酯的双组分聚氨酯粘合剂。双组分聚氨酯粘合剂的优点在于,其在混合之后即使在不提高的环境温度下也能迅速固化(“冷固化”)并因此在很短时间之后就已经能迅速承受较高的力。但是若要作为结构型粘合剂使用,则对此类粘合剂的强度和粘合力有很高的要求,因为这类粘合剂为承载结构的元素。通常通过高的交联密度实现高的强度。这通常通过提高官能基团的浓度并且使用较高官能度的多元醇或多胺以及较高官能度的多异氰酸酯来实现。
WO2006/084900A2公开了一种可以作为结构型粘合剂使用的双组分聚氨酯粘合剂。
但是尤其就风电装置转子叶片的构造而言(其中必须将预制的侧翼半壳与支撑结构粘合并且还必须将侧翼半壳相互粘合),迄今为止的双组分聚氨酯粘合剂具有很大的问题,即其必须具有较长的晾置时间,以便大面积涂覆粘合剂并且使得接合过程能够延迟发生。增大的空气湿度的存在会更多地导致异氰酸酯组分中的异氰酸酯基团与水发生副反应。在此过程中会消耗额外的异氰酸酯基团,这些异氰酸酯基团将无法再用来形成交联的聚氨酯。除此之外,所形成的二氧化钛还会使得粘合剂发泡。因此当例如在通常的季节变化时或者由于施工地点的特殊气候所能观察到的空气湿度较高时,粘合剂与空气水分的反应一方面尤其会大大缩短粘合剂的晾置时间,另一方面会使得固化后的粘合剂的机械特性严重变差。
WO2009/080740A1公开了一种双组分聚氨酯粘合剂,其适合用来粘合纤维成型件,其特征在于组合了高分子量的聚酯二醇、高官能度的多元醇、疏水性多元醇和其它助剂。但是这些粘合剂具有很高的刚性,其E-模量值大于2000 MPa,并且在机械性能上在改善机械韧性方面仍有改善能力。
将预制的侧翼半壳与支撑结构粘合时必然会出现接缝。除此之外,在较长时间使用结构粘合的转子叶片之后,还可能会在构件本身中或者在粘合接缝区域内形成可在表面上看见的缝隙形式的应力裂纹。为了填充这些接缝和缝隙,必须使用如上所述具有较长晾置时间和高机械强度并且有在粘弹性改性材料意义上的一定程度粘弹性的粘合剂。
发明详述
本发明的任务因此在于提供双组分的聚氨酯组合物,所述聚氨酯组合物一方面具有较长的晾置时间,并且在涂布在基材上之后和在于具有高空气湿度的气候下曝露较长时间之后(例如相对空气湿度70%),即使在40分钟之后、尤其即使在60分钟之后也能被接合(粘合)并且固化成为具有一定程度弹性(5~15%断裂伸长率)和高拉伸强度(>15MPa)的聚合物。
令人惊奇地已经发现,如下所述的双组分聚氨酯组合物能够解决这个问题。
已表明,这些组合物因为其机械特性而十分适合于在大面积成型件的结构粘合时填充接缝和缝隙,尤其适合于在建造风电装置时填充转子叶片-半壳的接缝和缝隙。有其表明,根据本发明的粘合剂在粘弹性改性材料意义上的断裂伸长率和拉伸强度之间具有特别好的平衡。
其它独立权利要求的主题是本发明的其它方面。从属权利要求的主题是本发明的特别优选的实施方式。
发明的实施方式
本发明涉及一种由多元醇组分(K1)和多异氰酸酯组分(K2)构成的双组分聚氨酯组合物。
在此,所述多元醇组分(K1)包括
蓖麻油(A0);
至少一种具有5~8个羟基的多元醇(A1);
至少一种基于蓖麻油或豆油且羟值为150~200mg KOH/g的聚醚多元醇和/或聚酯多元醇(A2-1)
以及至少一种基于蓖麻油或豆油且羟值为210~300mg KOH/g的聚醚多元醇和/或聚酯多元醇(A2-2)。
在此所述多异氰酸酯组分(K2)包括至少一种多异氰酸酯(B1)。
物质名称中的前缀“多/聚”,例如“多元醇”、“多异氰酸酯”、“聚醚”或“多胺”,在本发明中表示相应的物质在形式上每个分子包含一个以上在其名称中出现的官能基团。
在本发明中将结构粘合的转子叶片表面上可见的裂纹称作缝隙。
所述多元醇组分(K1)包括蓖麻油(A0)。蓖麻油是一种天然再生的原料,并从蓖麻灌木(Ricinus communi s,大戟种植物)的种子中获取。蓖麻油基本上是一种甘油三酸酯。蓖麻酸具有仲羟基。因此蓖麻油是一种疏水性多元醇。可以使用粗制或者提纯的蓖麻油。已证明特别适合的是使用具有减少的游离脂肪酸含量的蓖麻油(低FFA蓖麻油)。优选使用游离脂肪酸的含量小于重量5%、尤其在1~4重量%之间的蓖麻油。
在工业产品中使用作为可再生天然产物的蓖麻油从生态角度来看极其有价值的,因此非常有益。
蓖麻油(A0)在多元醇组分(K1)中的含量有利地在5~30重量%之间,尤其在10~25重量%之间,优选在14~20重量%之间。
多元醇组分(K1)包括至少一种具有5~8个羟基的多元醇(A1)。在粘合剂行业中通常很少使用此类高官能度的多元醇作为多元醇,因为其交联作用很强,并因此在多数体系中会在固化之后导致脆化。尤其适用的是糖醇以及基于糖醇的多元醇,其具有相应的羟基数,尤其是戊五醇或己六醇或者基于二糖的多元醇。也可以使用相应的糖,但尤其涉及加氢糖醇。例如有山梨醇、肌醇、甘露醇、阿东糖醇、核糖醇、木糖醇、卫矛醇、葡萄糖、半乳糖、甘露糖、阿洛糖、阿卓糖、古洛糖、艾杜糖、塔罗糖、果糖、山梨糖、阿洛酮糖、蔗糖、乳糖、海藻糖、麦芽糖、纤维二糖、蜜二糖以及芸香糖。也可以使用具有最多15个环氧烷单元的相应乙氧基化产物和丙氧基化产物。
具有5~8个羟基的这些多元醇(A1)的分子量可以为120~3000g/mol、尤其可以为250~2000g/mol。
也可以使用聚醚多元醇。为此的例子是5~6官能度的醇类的反应产物,其可以通过与环氧乙烷或环氧丙烷进行反应制备。
另一类适用的聚醚多元醇是聚四亚甲基二醇,尤其是例如可以通过四氢呋喃的酸聚合制备的聚(THF)二醇。在此,这些聚醚多元醇的分子量大体上在 200~6000g/mol之间,优选在400~3000g/mol范围内。
具有5~8个羟基的多元醇(A1)由于反应性羟基的高数量而具有较高的极性。它们因此至少部分地也可以与水混合。
具有5~8个羟基的多元醇(A1)优选基于山梨醇。具有5~8个羟基的多元醇(A1)特别优选地仅仅具有仲羟基。
具有5~8个羟基的多元醇(A1)在多元醇组分(K1)中的含量有利地在5~30重量%之间,尤其在0.5~20重量%之间,优选在1~10重量%之间。
多元醇组分(K1)包括至少一种基于蓖麻油或豆油且羟值为150~200mg KOH/g的聚醚多元醇和/或聚酯多元醇(A2-1)。优选羟值为155~190mg KOH/g。此外还优选具有300~400g/eq的羟基当量。
优选将蓖麻油与酮树脂的反应产物作为此类聚醚多元醇和/或聚酯多元醇(A2-1),尤其是例如由Bayer公司以名称1150和Cognis公司以名称805销售的产品。
所述多元醇组分(K1)包括至少一种基于蓖麻油或豆油且羟值为210~300mg KOH/g的聚醚多元醇和/或聚酯多元醇(A2-2)。优选的是羟值为215~270mgKOH/g。此外还优选其具有2.5~3、尤其2.6~2.9之间的羟基官能变。
优选将蓖麻油与酮树脂的反应产物作为此类聚醚多元醇和/或聚酯多元醇(A2-2)。
在此关键要实现,不仅需要存在多元醇(A2-1),而且也需要存在多元醇(A2-2),才能实现有利的特性。多元醇(A2-1)与多元醇(A2-2)的重量比有利地在8~1之间、尤其在5~1.5之间、优选在2~3之间。
此外,多元醇组分(K1)还优选包含其量为0.5~5重量%、优选1.5~2.5重量%的至少一种多胺(PA)。
适用的多胺(PA)是聚氨酯化工行业中常用的多胺,尤其是二胺。但是特别适用的是疏水性多胺,尤其是芳族多胺。特别优选的多胺(PA)是具有结构式(II)的芳族二胺:
式中R10、R11、R12和R13分别表示H或者直链或支化的C1~C4烷基,条件是R11和R13不同时表示H。此外R14和R15分别表示H或者氯原子。
尤其优选的是4,4′-亚甲基双(3-氯,2,6-二乙基)苯胺、4,4′-亚甲基双(3-氯-2,6-二乙基苯胺)、4,4′-亚甲基双(2,6-二乙基苯胺)、4,4′-亚甲基双(2,6-二异丙基苯胺)以及4,4′-亚甲基双(2-异丙基-6-甲基苯胺)。
与其它芳族多胺相比优选的是这类芳族多胺,因为其是毒理学上有利的芳族多胺。
特别优选的多胺(PA)是4,4′-亚甲基双(2,6-二乙基苯胺)。
多元醇组分(K1)还可以包括其它成分。有利地使用固化催化剂。对于多异氰酸酯与多元醇的反应,任选地也对于与多胺或水的反应,这类催化剂对于本领域技术人员而言是已知的。此类催化剂例如锡、锌和铋的有机金属催化剂,例如二月桂酸二丁基锡,或者叔胺,例如1,4-二氮杂双环[2.2.2]辛烷(DABCO)。
通过适用的多胺(PA)以及催化剂的选择和浓度,就能有利地影响组分(K1和K2)的混合物的适用期和固化特性以及粘度或者所涂布的粘合剂的稳定性。
尤其优选的是具有多元醇组分(K1)的双组分聚氨酯组合物,所述多元醇组分含有:
10~25重量%的蓖麻油(A0);
1~10重量%的具有5~8个羟基的多元醇(A1);
1~40重量%的基于蓖麻油或豆油且羟值为150~200mg KOH/g的聚醚多元醇和/或聚酯多元醇(A2-1)
1~30重量%的基于蓖麻油或豆油且羟值为210~300mg KOH/g的聚醚多元醇和/或聚酯多元醇(A2-2)。
多异氰酸酯组分(K2)包括至少一种多异氰酸酯(B1)。
特别适合作为多异氰酸酯(B1)的一方面是除了具有两个或更多游离异氰 酸酯基之外还具有至少一个脲基或者氨基甲酸酯基或者缩二脲基或者脲二酮基的多异氰酸酯(B1′)。
优选多异氰酸酯(B1)是芳族多异氰酸酯。尤其适合的是二苯基甲烷二异氰酸酯(2,4′-和/或4,4′-MDI)以及基于MDI的多异氰酸酯。一方面已证明如可从Bayer商购得到的名为VH20的那些类型的多异氰酸酯特别适用。此外适用的多异氰酸酯(B1′)还有二异氰酸酯,尤其是HDI和/或IPDI和/或TDI的异氰脲酸酯或者缩二脲。
完全可以使用多异氰酸酯B1′的混合物。
在一种优选实施方式中,使用单核和多核的MDI(所谓的聚合物MDI)的混合物。已证明Bayer的VKS20F特别适宜作为多异氰酸酯(B1)。
另一方面特别适合作为多异氰酸酯(B1)的是具有至少两个异氰酸酯基团的聚氨酯预聚物(B1″),并且其由至少一种分子量小于300g/mol、尤其在150g/mol~270g/mol之间的多异氰酸酯与至少一种多元醇(AB1)进行反应形成。特别适合作为多元醇(AB1)的多元醇选自聚醚多元醇、聚酯多元醇、聚碳酸酯多元醇、由不饱和单体及其混合物构成的多元醇。以已知的方式和方法制备具有此类异氰酸酯基团的聚氨酯预聚物,并且一般以多异氰酸酯对多元醇化学计量过量的量来进行。为此使用的多异氰酸酯尤其是2,4-和2,6-甲苯二异氰酸酯(TDI)、2,4′-和4,4′-二苯基甲烷二异氰酸酯(MDI)、1,6-六亚甲基二异氰酸酯(HDI)及其异构体混合物以及相互间的混合物。尤其优选的是MDI。
作为聚醚多元醇(也称作聚氧化亚烷基多元醇)的是环氧乙烷、1,2-环氧丙烷、1,2-或2,3-环氧丁烷、四氢呋喃或者其混合物的聚合产物,必要时它们借助于具有两个或更多活泼氢原子的起始剂分子进行聚合,例如水,氨或者具有多个OH或NH基团的化合物,例如1,2-乙二醇、1,2-和1,3-丙二醇、新戊二醇、二乙二醇、三乙二醇、异构的二丙二醇和三丙二醇、异构的丁二醇、戊二醇、己二醇、庚二醇、辛二醇、壬二醇、癸二醇、十一烷二醇、1,3-和1,4-环己烷二甲醇、双酚A、氢化双酚A、1,1,1-三羟甲基乙烷、1,1,1-三羟甲基丙烷、甘油、苯胺以及上述化合物的混合物。既可以使用具有低不饱和度(根据ASTM D-2849-69测得,且以每克多元醇的毫当量不饱和度(mEq/g)给出)的聚氧化亚烷基多元醇(例如借助于所谓的双金属氰化物络合催化剂(DMC-催化剂)制得),也可以使用具有更高不饱和度的聚氧化亚烷基多元醇(例如借助于阴离子 催化剂如NaOH、KOH或碱金属醇盐制得)。
特别适用的是聚氧化亚烷基二醇或者聚氧化亚烷基三醇,尤其是聚氧化亚丙基二醇或者聚氧化亚丙基三醇。
特别适用的是不饱和度低于0.02meq/g且分子量在1000~30000g/mol范围内的聚氧化亚烷基二醇或者聚氧化亚烷基三醇,以及分子量在400~8000g/mol之间的聚氧化亚丙基二醇和三醇。本发明所述的“分子量”或者“摩尔质量”始终指的是数均分子量Mn。
所谓的“EO-封端”(环氧乙烷封端的)聚氧化亚丙基二醇或者三醇同样也特别适用。后者是特定的聚氧化亚丙基聚氧化亚乙基多元醇,其例如通过在聚丙氧基化反应结束之后将纯的聚氧化亚丙基多元醇与环氧乙烷进行烷氧基化,并由此使其具有伯羟基而得到。
可作为聚酯多元醇的尤其是例如由二元至三元醇与有机二羧酸或者其酸酐或酯制备的多元醇,所述二元至三元醇例如1,2-乙二醇、二乙二醇、1,2-丙二醇、二丙二醇、1,4-丁二醇、1,5-戊二醇、1,6-己二醇、新戊二醇、甘油、1,1,1-三羟甲基丙烷或者上述醇的混合物,所述有机二羧酸例如琥珀酸、戊二酸、己二酸、辛二酸、癸二酸、十二烷二羧酸、马来酸、富马酸、邻苯二甲酸、间苯二甲酸、对苯二甲酸和六氢邻苯二甲酸或者上述酸的混合物,以及由内酯例如ε-己内酯得到的聚酯多元醇。
作为聚碳酸酯多元醇,尤其优先的是通过上述的用于构建聚酯多元醇的醇与碳酸二烷基酯、碳酸二芳基酯或者光气进行反应而获得的那些。
作为““由不饱和单体形成的多元醇”尤其理解为由至少一种单体的聚合制备的多元醇,所述单体选自:乙烯、丙烯、丁烯、丁二烯、异戊二烯、苯乙烯、乙烯基醇、乙烯基醚、乙烯基酯、丙烯腈,丙烯酸、甲基丙烯酸、马来酸、富马酸、巴豆酸和衣康酸的酸、酰胺和酯及其混合物。
作为由不饱和单体所形成的特别适用的多元醇的是羟基官能的聚丁二烯,如聚丁二烯多元醇和氢化聚丁二烯多元醇以及聚(甲基)丙烯酸酯多元醇。本发明在这里和下文中,所述的“(甲基)丙烯酸酯”始终理解为丙烯酸以及甲基丙烯酸的酯。“(甲基)丙烯酸”同样不仅指丙烯酸,而且也指甲基丙烯酸。
在此,作为“聚(甲基)丙烯酸酯”理解为是羟基官能的(甲基)丙烯酸酯与至少一种其他单体的共聚物的聚合物,所述其他单体选自:丙烯酸、甲基 丙烯酸、丙烯酸或甲基丙烯酸的C1-C18-烷基酯、苯乙烯、乙烯基酯和乙烯基醇。优选(甲基)丙烯酸羟乙基酯、(甲基)丙烯酸羟丙基酯和(甲基)丙烯酸羟丁基酯作为羟基官能的(甲基)丙烯酸酯。
这些提及的多元醇(AB1)的平均分子量优选为250~30000g/mol、特别为1000~8000g/mol并且优选是二醇或三醇,特别是平均羟基官能度在1.6~3范围内的二醇或三醇。
在一种优选实施方式中,使用多元醇(AB1)的混合物,该混合物是二醇和三醇的混合物。
在本发明的一种实施方式中,多异氰酸酯组分(K2)包含至少一种多异氰酸酯(B1′)和至少一种多异氰酸酯-聚氨酯预聚物(B1″)。
多元醇组分(K1)和/或多异氰酸酯组分(K2)除了已经提及的之外,还可以具有其他成分,如双组分聚氨酯化工行业的专业人士熟知的那些。它们可以仅仅存在于其中一个组分中,或者可以存在于两个组分中。作为此类附加的成分例如有:溶剂、增塑剂和/或增量剂填料,如炭黑、白垩或滑石、增附剂,尤其是三烷氧基硅烷,以及触变剂如无定形硅酸,和干燥剂如沸石。
正如专业人士对于聚氨酯粘合剂所知道的那样,在制备组分,尤其在制备多异氰酸酯组分(K2)时必须注意:原料尽可能没有水并且在其制备过程中和制备后尽可能不要有水分与组分接触。这一方面通过物理或化学干燥初始物质以及通过在惰性气体(通常是氮气)或者在真空条件下操作来实现。
有利地如此配制组分(K1,K2),使得多元醇组分(K1)和多异氰酸酯组分(K2)的体积比在1:3~3:1之间、尤其在1:2~2:1之间。该比例尤其优选大致为1:1。优选混合比是这样的,即使得多异氰酸酯组分(K2)的NCO基团对于多元醇组分(K1)的NCO反应性基团(通常是羟基)是按照化学计量比的。如果没有基本上按照化学计量比进行混合,即如果偏差大于5重量%,则多元醇组分(K1)与多异氰酸酯组分(K2)就不会最佳地进行反应,这导致经固化的聚氨酯组合物的机械性能降低。这主要适于多元醇组分过量的情况。如果存在过量的多异氰酸酯,则尽管这在原则上同样是不利的,但是由于未转化的异氰酸酯基团后续与水分,例如空气湿气主导的水气的反应(这可能会导致进一步的交联),因此能够至少部分弥补聚氨酯网络结构中的缺陷以及因此导致的变差的机械性能。
在使用之前彼此分开地存放多元醇组分(K1)和多异氰酸酯组分(K2),并且只有当使用时或者即将使用之前才将其相互混合。有利地这些组分存在于由两个相互隔开的腔室构成的包装之中,使得多元醇组分(K1)存在于其中一个腔室之中,而多异氰酸酯组分(K2)则存在于另一个腔室之中。将多元醇组分(K1)和多异氰酸酯组分(K2)填充入包装的腔室之中,然后将其密闭隔绝空气和水分。
优选的此类包装一方面是并列双料盒或者同轴料盒,其中的两个管状腔室并排或者叠套布置并且利用活塞隔绝空气和水分而密封。经由前推该活塞就可以将组分从料盒中挤出。必要时通过适配器如此改进与活塞相对的管侧面,使得在开口区域中通过隔壁将腔室开口直接相互连接。在腔室的出口区域中有利地安置螺纹,使得可以密闭安装静态混合器或者动态混合器。尤其对于填装量至多1升的小型应用而言,此类包装是尤其优选的。
对于比较大型的应用,尤其是工业生产中的应用,有利地将多元醇组分(K1)和多异氰酸酯组分(K2)填装在桶或者提桶之中并存放。这种情况下通过液压机、尤其通过后续压盘(Folgeplatten)将组分压出,并通过管道输送给诸如通常在工业生产中用于双组分粘合剂的混合装置。
无论采用何种包装,重要的是至少将多异氰酸酯组分(K2)隔绝空气和水分地密封,使得两种组分可以在长时间内存放,即通常存放6个月以上。
双组分的聚氨酯组合物有利地是能够流动的,但是在此尤其也可以具有触变性能。经固化的双组分聚氨酯组合物具有很高的机械强度,尤其具有很高的拉伸强度值(在本发明中始终使用断裂点处的应力值),相据ISO527-2在接合之后立即进行测定,具有大于12MPa、优选大于15MPa以及最优选大于20MPa的该值。但是该拉伸强度通常小于40MPa。此外,经固化的双组分聚氨酯组合物还具有根据ISO527-2测量的5~15%、尤其在8~12%之间的断裂伸长率。
因此经固化的双组分聚氨酯组合物具有非常高的机械强度,其容许使用双组分聚氨酯组合物作为用于结构粘合的粘合剂和用于填充结构粘合中的接缝和缝隙,特别是风电装置转子叶片的接缝和缝隙。
本发明另一方面涉及一种以力锁合方式(kraftschlüssigen)填充基材中的接缝和缝隙的方法,包括以下步骤:
a)将双组分聚氨酯组合物的多元醇组分(K1)与多异氰酸酯组分(K2)混合,与之前详细描述的那些,
b)将混合后的聚氨酯组合物施涂到两个甚材之间待弥补的接缝中,或者施涂到基材表面上待填充的缝隙之中,
c)将在接缝或者缝隙中的聚氨酯组合物固化。
按照所述的顺序执行这些步骤。
通常通过静态混合器或者利用动态混合器进行混合。在混合过程中要注意将两种组分尽可能均匀混合。如果两个组分不完全混合,就会出现局部偏离最佳混合比的情况,也就是基本上偏离最佳化学计量比,从而使得经固化的聚氨酯组合物的机械性能变差。为了也能目测评估混合质量,多元醇组分(K1)和多异氰酸酯组分(K2)优选具有可以相互地、但也可以从混合物目视区分开来的两种不同的颜色。例如当其中一个组分为黑色并且另一个为白色时,就存在这样的颜色组合。如果存在均匀的灰色并且没有浅灰、深灰、白色或黑色的条纹和花样,则存在良好的混合。
将经混合的聚氨酯组合物施涂到接缝之中。在粘合大面积成型件的时候必然会产生这样的接缝。其主要原因是大的基材的尺寸误差。聚氨酯组合物必须能够尽可能广泛地填充接缝并且以力锁合方式将部件相互连接。这同样也适用于填充缝隙,该缝隙在较长时间使用结构粘合的转子叶片之后,在构件本身或者粘合接缝区域内会由于出现应力裂纹而能够在表面上看见。
可以利用喷嘴将组合物压入到接缝或缝隙之中,或者利用抹刀将组合物抹入到接缝或缝隙之中。因此粘合剂有利地具有一定的形状稠度。在此,其不应当过于稀液态,但是也不要过粘。已发现最佳的是:混合后的聚氨酯组合物具有类似于油灰的糊状稠度,稳定的并且有利地是剪切稀释性的,也就是可以手工涂抹。为了不必使用太多的混合的聚氨酯组合物,或者为了不必后续再重新去除涂覆得太多的聚氨酯组合物,可以有利地使用覆盖带或者临时附着的薄膜来遮盖接缝或缝隙的边缘。
形成待弥补的空隙的基材优选是金属、塑料、玻璃或陶瓷或者纤维复合材料。可以存在相互粘合的两种不同的基材。配对接合件(即第二基材)可以与第一基材相同或者不同。
通常在用于接合两个基材的粘合剂已经固化之后进行填充。
在用于填充的聚氨酯组分固化之后,可以其接缝或缝隙被填充的连接件进行机械后加工。这尤其包括抛充和打磨。所述后加工保证了获得最终形状,尤其是获得最佳立体形状。特别在制造风电装置的转子叶片的过程中,存在最佳的立体形状和表面特性尤其重要,因为这对转子叶片的空气动力学特性以及因此直接地对效率有很大影响,使得存在最佳立体形状和表面特性将会直接影响从风力获取的机械能的量和间接还有获取的电能的量。因此这是一个重要的经济和生态因素。
优选的基材是塑料,尤其是纤维增强的塑料。
此类纤维增强的塑料是嵌入到塑料构成的基质之中的纤维所构成的复合材料。
这些纤维增强塑料的合适的纤维选自如下列表的纤维:无机纤维(尤其是玻璃纤维和陶瓷纤维)和有机纤维。所述有机纤维优选是芳纶纤维、聚酯纤维、尼龙纤维、树脂玻璃纤维、乙烯和/或丙烯的均聚物或共聚物构成的纤维、天然纤维、纺织纤维和碳纤维。最优选的是碳纤维。
在此,所述纤维可以是短切纤维或长纤维,经纺的、经织造或非织造的纤维或长丝。此外所述纤维还可以是经定向或者拉伸的纤维。此外还可以有利地彼此使用不仅几何形状不同而且组成也相互不同的纤维。尤其使用这些纤维作为纺织物、铺织物或针织物或者毛毡或无纺布或者粗纱。通过塑料基质填充纤维之间存在的间隙。适用的塑料基质选自如下列表:环氧树脂、不饱和聚酯树脂、乙烯基酯树脂、酚醛树脂、邻苯二甲酸二烯丙酯树脂、(甲基)丙烯酸酯树脂、聚氨酯、氨基树脂、三聚氰胺对脂和脲树脂。尤其优选环氧树脂作为塑料基质。
特别优选的待粘合基材是基于聚酯或者聚环氧化物基质中的玻璃纤维和/碳纤维的成型件。可以按照已知的方式和方法,由聚酯或聚环氧化物以及玻璃纤维和/或碳纤维通过各种不同的工艺制备此类成型件。例如可将此类成型件用于飞机制造、船舶制造,或者用于其它机械负荷很高的构件。风电装置的转子叶片是此类粘合基材的一个特殊应用领域。此类成型件的制备方法是技术人员已知的。
例如在空心模具中生产风电装置的转子叶片并将其固化。在此通常将模具设计成半边的模具。一般来说,所得到的朝向模具的一侧为光滑的设计成即可 使用的表面,另一侧则可以并且通常应当还要进行加工。在此,在侧翼的下一步生产过程中将两个或者更多的基材相互粘合。还可通过置入支撑结构的方式对侧翼进行机械加固。在此粘合剂保证半壳形状与支撑结构的连接。一般来说,将背向模具的一侧用作为待粘合的侧面。表面应当优选如此来设计,使得待粘合的基材部分近似具有配合形状。设计为待粘合的表面可以是粗糙、本身不平整的。不需要打磨或者铣削成与待粘合的配合件呈精确的镜像形状。没有粉尘和油脂的表面足以涂覆粘合剂,不需要使用底漆。
已知的一种操作方法是在模具中制成用于交联(Vernetzung)的部件之后使用抗撕裂的防护织物来遮盖成型件的外侧表面。可以在快要进行稍后粘合之前将其完全撕去,从而产生合适的表面。但是也可以用机械方式粗糙处理这些表面并且使其适应于相应的配合件。然后就可以将粘合剂涂布在经过如此预处理并且去除了松散部件和粉尘的基材表面上。然后与之前所述的一样,使用双组分聚氨酯组合物填充通过粘合接合的成型件之间剩余的接缝或者缝隙。
但是双组分聚氨酯组合物由于其机械特性也完全可以作为粘合剂使用。
因此本发明的另一方面同样也涉及一种粘合方法。该方法包括以下步骤:
a′)将双组分聚氨酯组合物的多元醇组分(K1)与多异氰酸酯组分(K2)混合,如之前详细描述的那些,
b′)将经混合的聚氨酯组合物施涂到至少一个待粘合的基材表面上,
c′)在晾置时间内接合,
d′)将聚氨酯组合物固化。
所述双组分聚氨酯组合物的晾置时间特别适合于粘合大型接合件或成型件,或者适合于填充大型接合件或成型件的接缝或缝隙。晾置时间表示这样的时间段:在该时间段内在混合两个组分并且随后施涂粘合剂之后,在粘合剂已经反应结束使得其不再能构造粘合连接体之前仍能使基材部分接合。
根据ISO11357测定,利用根据本发明的经固化的组合物能够获得超过50℃、尤其超过55℃的玻璃化转变温度。
通常在室温和50重量%的相对空气湿度条件下,双组分聚氨酯组合物的晾置时间大于60分钟、尤其在60分钟和4小时之间。
本发明的一个特别大的优点在于,即使空气湿度较大,例如70重量%的相对空气湿度,晾置时间仍然很长,也就是至少60分钟。因为已知的异氰酸酯 对水、尤其是来自空气湿气的水分的反应性,这对于专业人士而言必然十分令人意外。
该特性允许基本上不论空气湿度而可靠地实现大面积地粘合或者填充大型成型件的接缝或缝隙,例如风电装置的转子叶片制造车间中出现的或者现场修补缝隙时出现的那些。当然在此重要的是机械性能不会由于高空气湿度而受到严重不利的影响。
由上述方法得到制品,尤其是风电装置的转子叶片。
上述的双组分聚氨酯组合物因此特别适合用作粘合剂,尤其适合用作结构型粘合剂,尤其作为在风电装置的转子叶片制造过程中的力传递结构单元。在建筑业、汽车、机动车或者船舶或风电装置中可以找到此类粘合剂的典型应用示例。在此,经固化的粘合剂是承载结构的一部分并因此构成重要的连接部分,对其机械性能提出了很高的要求。本发明能最佳地满足这些高要求。
上述双组分的聚氨酯组合物尤其适合用作接缝或缝隙的填充剂,尤其适合作为风电装置转子叶片制造或维修过程中的力锁合的填充材料。
实施例
以下实施例用于阐述本发明:但是这些实施例应不视作对本发明具有限制作用。
表1中举例列出的组合物1和作为参考实施例的Ref.1~Ref.4均具有相同的组分K2。
为制备组分K1,在真空分散机中预置入多元醇混合物,和在加入催化剂和干燥剂之后在25℃下隔绝水分搅拌20分钟。接着将这些多元醇组分K1填装到隔绝空气和水分的料盒之中。
对于组分K2,将多异氰酸酯组分B1填装到隔绝空气和水分的料盒中。
按照如表1所示的K1:K2的重量比利用静态混合器混合组分K1和K2(对应于NCO/OH比例为1.1)。
测量
E-模量、拉伸强度和断裂伸长率
混合经混合的组分K1和K2,并且在混合之后立即按照ISO527第2部分1B(ISO527-2)制作哑铃形试样,在25℃温度下使其固化24小时和接着 在60℃温度下固化72小时。在25℃温度下经过24小时调理之后,按照ISO527-2在Zwick Z020拉伸测试机上在20℃的测试温度下和采用2 mm/min的测试速度测定如此制得的试样体的拉伸强度、E-模量和断裂伸长率。
拉伸剪切强度
混合经混合的组分K1和K2,并将其施涂到玻璃纤维增强的环氧树脂(GRE)的第一个薄板上。接着,立即或者在25℃和70重量%相对空气湿度条件下曝露40或60分钟之后(texp)继续制作拉伸剪切强度试样体(与第二个玻璃纤维增强的环氧树脂薄板接触,挤压,粘合剂厚度2mm)。然后使粘合剂在25℃温度下固化24小时并接着在60℃温度下固化72小时,在于25℃温度下经过24小时调理时间之后根据ISO 527测定拉伸剪切强度。
表1组成和测量结果
1rel.LF=相对空气湿度
2聚酯/聚醚,基于羟值为220~260mg KOH/g的蓖麻油,官能度:2.8
3GT=重量份
实施例1和Ref.2的对比表明,不存在具有5~8个羟基的多元醇会导致拉伸强度不适当地强烈下降并且会导致断裂伸长率显著升高。此外拉伸剪切强度同样也令人惊讶地严重变差。
实施例1和Ref.1的对比表明,同时存在的基于蓖麻油或豆油的聚醚多元醇和/或聚酯多元醇(A2-1)和(A2-2)的重要性。如果不存在基于蓖麻油且羟值较高的聚醚多元醇和/或聚酯多元醇,那么在潮湿空气中经过较长的晾置时间之后,尤其经过60分钟之后,拉伸剪切强度就会出乎意料地急剧变差。
即使在Ref.3和Ref.4中,在潮湿空气中经过较长的晾置时间之后,尤其经过60分钟之后,拉伸剪切强度也会出乎意料地急剧变差。
实施例1表明采用根据本发明的组合物一方面能够在填充剂所需的断裂伸长率与拉伸强度之间实现恰当的平衡,另一方面即使在经施涂的聚氨酯组合物在潮湿空气中暴露较长时间之后仍能可靠地构建粘附力,并从而能够在填充剂与基材之间的边界层中实现力锁合性的形状缩合。
Claims (17)
1.由多元醇组分(K1)和多异氰酸酯组分(K2)构成的双组分聚氨酯组合物;
其中所述多元醇组分(K1)包含
蓖麻油(A0);
至少一种具有5~8个羟基的多元醇(A1);
至少一种基于蓖麻油或豆油且羟值为150~200mg KOH/g的聚醚多元醇和/或聚酯多元醇(A2-1);
以及至少一种基于蓖麻油或豆油且羟值为210~300mg KOH/g的聚醚多元醇和/或聚酯多元醇(A2-2);
并且其中所述多异氰酸酯组分(K2)包含至少一种多异氰酸酯(B1)。
2.根据权利要求1所述的双组分聚氨酯组合物,其特征在于,具有5~8个羟基的多元醇(A1)是仅仅具有仲羟基的多元醇。
3.根据权利要求1所述的双组分聚氨酯组合物,其特征在于,具有5~8个羟基的多元醇(A1)是基于山梨醇的聚醚多元醇。
4.根据权利要求1~3中任一项所述的双组分聚氨酯组合物,其中所述多异氰酸酯(B1)是芳族多异氰酸酯。
5.根据权利要求1~3中任一项所述的双组分聚氨酯组合物,其特征在于,多元醇组分(K1)还含有其量为0.5~5重量%的多胺。
6.根据权利要求5所述的双组分聚氨酯组合物,其特征在于,多元醇组分(K1)还含有其量为1.5~2.5重量%的多胺。
7.根据权利要求1~3中任一项所述的双组分聚氨酯组合物,其特征在于,所述多元醇组分(K1)含有:
10~25重量%的蓖麻油(A0);
1~10重量%且具有5~8个羟基的多元醇(A1);
1~40重量%的基于蓖麻油或豆油且羟值为150~200mg KOH/g的聚醚多元醇和/或聚酯多元醇(A2-1);
1~30重量%的基于蓖麻油或豆油且羟值为210~300mg KOH/g的聚醚多元醇和/或聚酯多元醇(A2-2)。
8.以力锁合方式对基材中的接缝和缝隙进行填充的方法,包括以下步骤:
a)将根据权利要求1~7中任一项的双组分聚氨酯组合物的多元醇组分(K1)与多异氰酸酯组分(K2)混合,
b)将经混合的聚氨酯组合物施涂到两个基材之间待弥补的接缝之中或者施涂到基材表面上待填充的缝隙之中,
c)将接缝或者缝隙中的聚氨酯组合物固化。
9.粘合方法,包括以下步骤:
a')将根据权利要求1~7中任一项的双组分聚氨酯组合物的多元醇组分(K1)与多异氰酸酯组分(K2)混合,
b')将经混合的聚氨酯组合物施涂到至少一个待粘合的基材表面上,
c')在晾置时间之内进行接合,
d')将聚氨酯组合物固化。
10.根据权利要求9所述的方法,其特征在于,所述待粘合的基材是塑料。
11.根据权利要求9所述的方法,其特征在于,所述基材是纤维增强的塑料。
12.根据权利要求8~11中任一项所述方法获得的制品。
13.根据权利要求12所述的制品,其特征在于,所述制品是风电装置的转子叶片。
14.根据权利要求1~7中任一项的双组分聚氨酯组合物的用途,作为粘合剂。
15.根据权利要求1~7中任一项的双组分聚氨酯组合物的用途,作为结构型粘合剂。
16.根据权利要求1~7中任一项的双组分聚氨酯组合物的用途,作为用于接缝或缝隙的力锁合型填充剂。
17.根据权利要求14或15或16所述的用途,作为在风电装置的转子叶片制造过程中力传递的结构单元。
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PCT/EP2011/073411 WO2012084949A1 (de) | 2010-12-24 | 2011-12-20 | Klebstoff für das verfüllen von fugen und spalten in rotorblättern für windkraftanlagen |
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